以KF和Al(NO3)3·9H2O为反应物,采用乙二醇回流法合成了纳米复合氟化物KAlF4,考测了反应物的选择、配比、反应时间等因素对产物的影响,并利用XRD、TEM 、XPS等技术对其结构、形貌、粒径以及表面氧含量进行了表征.结果表明,采用回流法在适当的反应条件下合成的KAlF4具有单一相结构的复合氟化物,平均粒径为32.5 nm,属于纳米颗粒,合成的产物不含晶格氧,仅有吸附氧且含量较低该方法具有工艺简单、反应时间短、不腐蚀设备、不需要煅烧直接生成晶相等优点,具有广阔的开发应用前景.%Nano complex fluoride KAlF4 particles were synthesized by refluxing method using KF and Al(NO3)3 · 9H2O as reactants in ethanediol ,and different synthesis conditions such as reactants, ratio of reactants and reaction time were studied in the paper. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) , X-ray electron spectroscopy (XPS). The results show that single crystalline phase of KAlF4 can be obtained under the appropriate reaction conditions by reflux method,and the mean diameter of particles KAlF4 is approximately 32.5nm. Only ehemi-adsorption oxygen (α oxygen) exists on the surface of KAlF4 in the O1s XPS peak spectra of KAlF4. The reflux method has many advantages such as simple process, mild conditions, fast phase-transformation rate, and so on. The method has a broad development prospect in the future.
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